Process of making varnish-gum.



UNITED STATES PATENT ()FFIGE.

Specification of Letters Patent.

Patented Sept. 12, 1905.

Application filed January 21,1901. Serial No. 44,179.

To all whom, it mag concern:

Be it known that I, ABRAHAM KRoNsTuIN, chemist, a subject of the Emperorof Austria- Hungary, residing at 95 Kriegsstrasse, in the city ofKarlsruhe, in the Grand Duchy of Baden, German Empire, have invented acertain new and useful Process of Making Varnish-Gums, of which thefollowing is a specification.

In a previous application for United States Letters Patent I have shownthat under certain conditions solid substances will be obtained fromdrying-oils, the said substances being insoluble in the ordinarysolvents of the resins and oils. This quality is in particular possessedby mixtures which contain more than (fifty per cent.) of wood-oil. Ihave now found that these solid bodies which are insoluble in theordinary solvents of resins, oils, and balsams may also be obtained fromwood-oil which has been mixed with acertain amount of resins, and it hasbeen found that according to the nature of the particular kind of resindifferent quantities of the same will be necessary to produce thesolidification of the wood-oil. It seems that the amount of volatile oilpresent in the resin influences the solidification process.

The solubility of the product obtained by heating liquid wood-oil withresins depends besides on the nature of the resin, also upon theduration of the heating process. If suflicient resin is added toso-called Chinese wood-oil or tung-oil, being the oil of Elm 000cm warnJoell or rllem'z zes corridor, in a liquid state and the mixture heatedat an elevated temperature for a sufficient length of time, preferably,though not necessarily, at the exclusion of air, the mixture becomesviscid and finally solidifies. This solidification takes place duringthe heating process itself and yields substances which are a perfectsubstitute for the expensive gum-copal and amber and they show the sameproperty of being insoluble in all solvents. These solid products showan approximate melting-point of from about 280 to 350 centigrade. Thebrittleness of the resins has been entirely lost in the new products,which show a high degree of elasticity, and like the ordinary hardresins of nature only become soluble if remelted at a highertemperature. In this con dition they are soluble in oil of turpentine,benzol, and camphor-oil. If the new products are melted, they yield athick oil which is soluble in the ordinary solvents and is suitable foruse in the manufacture of japans and varnishes.

If a greater quantity of resin is added to the wood-oil than isnecessary for solidification at a temperature of about 200 centigrade,the mixture loses the property of becoming solid and insoluble duringthe heating process itself. These mixtures, on the contrary, remainliquid during the heating process and only when cooled down they yieldat ordinary temperature solid resinous bodies which are distinguished bya high degree of elasticity and which are soluble in the ordinarysolvents, such as oil of turpentine, benzol, and camphor-oil.

In apply ng my invention to the resins and gums of commerce it has beenfound that an addition of as much as fifty per cent. of gumdammar doesnot yet prevent the solidification of wood-oil during the heatingprocess. About the same percentage applies to the use of Venetianturpentine, and the limit is very near the same for melted amber,guttapercha, and asphaltum, while if copal is used as an admixture thepercentage may be as high as seventy per cent; on the other hand, ofresin or colophony only about thirty per cent may be added for producingthe same effect. I may also use mixtures of different kinds of resinsfor producing a solidification and the formation of insoluble bodiesduring the heating process. I may also make use of additions ofdrying-oils--such as linseed-oil, rape-seed oil, cotton-oil, and ofsimilar oilsto the resins and mix these with the wood-oil. The formationof such solid, insoluble, and elastic products from resins is due topolymerization of the wood-oil, the limit at which polymerization takesplace depending, of course, in each case upon the nature of the mixtureof the resin or of mixtures of different kinds of resin withdrying-oils. There will, however, be a certain limit of temperatu re andof percentage for each mixture, which has to be found by experience. Thethus-obtained products, which, as aforesaid, are perfect substitutes forthe expensive hard rosins used heretofore, may be employed in themanufacture of japans and varnishes and for electrical purposes for themanufacture of insulating material, cable-wax, and the like.

It is preferable to avoid the access of air in order to exclude thepossibility of decompo sition and in order to obtain pure light-coloredproducts. On the other hand, if the process is carried on under accessof air, oxi- IIO dation and decomposition will take place, giving riseto the formation of colored products ofinferior quality. if the heatingprocess is interrupted before solidification sets in, the

process only yields an oil which is still soluble in the ordinarysolvents and is suitable for use in the manufacture of japans andvarnishes. The mode of procedure to' be followed in carrying out myinvention will be illustrated by the following examples:

Example 1: Eighty pounds of dammarresin are dissolved in one hundred andtwenty pounds of wood-oil and are then heated up to about 200 to 250centigrade. The solution solidifies afterthe heating process has gone onfor about sixteen to eighteen hours, solidification setting in duringthe heating process itself and yielding a product which is insoluble inoil of turpentine, benzol, and the like. In these products the resinousconstituent has lost its brittleness and becomes so intimately combinedwith the wood-oil that it will not be directly acted upon by alkalies,as is the case in mechanical mixtures of dryingoils and resin orcolophony or other resins or in such mixtures where the resin was addedto the solidified and afterward molten wood-oil. By my invention Iobtain bodies which will not be attacked by alkalies under ordinaryconditions and which must be fused before they become open to the actionof any solvents or reagents. If the temperature is raised up to about800 centigrade, the product melts and yields an oil which is soluble inoil of turpentine, benzol, and the like; yield, theoretical.

Example 2: Forty pounds of resin are dissolved in one hundred and sixtypounds of wood-oil and treated as shown with reference to Example 1.

Example 3: A mixture of each forty pounds of dammar-resin andlinseed-oil are dissolved in one hundred and twenty pounds of woodoiland treated in like manner as in Example 1.

If the heating is interrupted before solidification takes placein theexamples mentioned under 1 to 3, the process yields soluble productswhich are of a very high consistency and even solid at ordinarytemperature and which are of importance in the manufacture of japans andof linoleum.

The effects of the useof an excess of resin will be illustrated by thefollowing examples:

- Example 4: One hundred and twenty pounds of dammar -resin aredissolved in eighty pounds of Wood-oil and heated for twenty-four hours.The product is solublein oil of turpentine, benzol, and the like andyields rapidly-drying japans.

Example 5: A mixture of each sixty pounds of amber and linseed-oil isdissolved in eighty pounds of wood-oil and is, forinstance, heated fortwenty-four hours. The product is solulbLe in oil of turpentine,camphor-oil, and the same quality as that obtained in Example 5. 1 amaware that it is old to produce a sub-' stitute for varnish-gum from amixture of ordlnary resln and wood-oil or tung-oll with or without theaddition of hardeningand drying chemicals; but in the former processreferred to the solidification of the mixture was produced by allowingthe heated mixture to cool and harden, whereby a product was obtainedwhich could be melted at a low temperature and did not withstand theaction of alkaliesand which even in the presence of the majority ofsolidification promoting chemicals as treated by the former process wasalso soluble in the ordinary solvents of resins and oils, while-in myinvention the product obtained which is insoluble and proof against theaction of alkalies andfuses at a very high temperature only is produced,so to speak, by a kind of coagulation at very high heat and not by thecooling of a liquid. Besides, the former proc ess was limited to the useof resin only and could not be employed with other kind of resins, whilemy process applies to any kind of resins as well, including hard resinsor natural.

varnish-gums,such as gum-dammar and copalgum also, and in my process noexcess of resin and no previous liquefaction of the same or of otherresins employed is necessary and no more resin is employed in themixture than is necessary to prevent the liquefaction of the Woodoil ortung-oil during the heating process.

What I claim, and desire to secure by Letters Patent of the UnitedStates, is-

1. The process for increasing the consistency of wood-oil or tung-oilsubstantially as described and for manufacturing artificial varnish-gumswhich consists in heating a mixture of a sufficiency of any suitableordinary commercially pure resin with wood-oil and continuing theheating until the liquid coagulates and solidifies and becomes insolubleduring the heating process and allowing the solid product obtained tocool.

2. The process for increasing the consistency of wood-oil or tung-oiland for manufacturing therefrom solid substitution products forvarnish-gums which consists in mixing ordinary resin with an excess ofwood-oil or tung oil substantially as described and heating the mixtureuntil it solidifies during the heating process and then interrupting theheating and allowing the solid product obtained to cool.

3. The process for increasing the consistency of wood-oil or tung-oil,substantially as described and for manufacturing artificial varnish-gumswhich consists in heatinga mixture of said wood-oil or tung-oil with anysuitable ordinary commercially pure resin the amount of which isgoverned by the volatile constituents of the resin, to a temperature ofabout 1 5200 to 250 centigrade and continuing the i heating, untiltheliquid coagulates and solidifies and becomes insoluble during theheating process and allowing the solid product obtained to cool.

4. The process for treating wood-oil or tungoil with resins whichconsists in mixing an excess of liquid wood-oil with a suitable amountof resin, adding drying-oils and heating the l mixture to a temperatureabout or above 200 i Centigrade until solidification sets in.

5. As a new product an alkali-resisting solid compound consisting of aninsoluble, difli cultly-fusing mixture of wood-oil or tung-oil and resinand having an approximate melting-point of from 280 to 350 centigrade.

In witness whereof I have hereunto signed my name in the presence of twosubscribing witnesses.

ABRAHAM KRONSTEIN. \Vitnesses:

HENRY HAsPER, VOLDEMAR HAUP'I.

